CN115891355A - Fluorine-based composite film and reinforcing plate - Google Patents
Fluorine-based composite film and reinforcing plate Download PDFInfo
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Abstract
Description
技术领域technical field
本发明属于FPC(柔性线路板)技术领域,特别是涉及一种氟系复合膜及补强板。The invention belongs to the technical field of FPC (flexible circuit board), in particular to a fluorine-based composite film and a reinforcing board.
背景技术Background technique
随着信息技术的飞跃发展,印刷电路板是电子产品中不可或缺的材料,而随着消费性电子产品需求增长,对于印刷电路板的需求也是与日俱增。由于软性印刷电路板(FPC,Flexible Printed Circuit)具有可挠曲性及可三度空间配线等特性,目前FPC被广泛应用计算机及其外围设备、通讯产品以及消费性电子产品等等。With the rapid development of information technology, printed circuit boards are an indispensable material in electronic products, and as the demand for consumer electronics grows, the demand for printed circuit boards is also increasing day by day. Due to the flexible printed circuit board (FPC, Flexible Printed Circuit) has the characteristics of flexibility and three-dimensional space wiring, FPC is currently widely used in computers and their peripheral equipment, communication products, and consumer electronics products.
在产品使用过程中,FPC的表面磨损是影响其使用寿命长短的重要因素之一,而材料的吸水率也会影响产品性能的有效发挥,所以寻求高耐磨损和低吸水率的材料用于FPC以提高产品使用寿命及高效能。In the process of product use, the surface wear of FPC is one of the important factors affecting its service life, and the water absorption rate of the material will also affect the effective performance of the product performance, so it is necessary to seek materials with high wear resistance and low water absorption rate for use. FPC to improve product life and high performance.
氟系树脂置于最外层时,其表现出较好的耐磨损性能,可以起到良好地保护作用,并且氟系树脂具有约为0.03%的低吸水率的优异性质,可以将空气中的水汽完美的隔绝在外,以保护内层材料,降低整体的吸水率。When the fluorine-based resin is placed on the outermost layer, it exhibits good wear resistance and can play a good protective role, and the fluorine-based resin has an excellent property of low water absorption of about 0.03%, which can absorb water in the air The water vapor is perfectly isolated to protect the inner material and reduce the overall water absorption.
然而,氟系树脂其高热膨胀系数(约200ppm/℃)易造成尺寸安定性不佳。此外,氟系树脂受到制程技术的限制,对制造设备的要求高且需要在较高温环境(>280℃)下才可以操作,随之也造成了其膜厚不均匀;此外,又面临了PTFE多为片状不能使用卷对卷的压合工艺,导致加工困难、量产性低、耗材更多。However, the high thermal expansion coefficient (about 200ppm/°C) of fluorine-based resins tends to cause poor dimensional stability. In addition, fluorine-based resins are limited by the process technology, which requires high manufacturing equipment and can only be operated in a relatively high temperature environment (>280°C), which also causes uneven film thickness; in addition, it is also faced with PTFE Most of them are in sheet form and cannot use the roll-to-roll lamination process, resulting in difficult processing, low mass production, and more consumables.
发明内容Contents of the invention
本发明主要解决的技术问题是提供一种氟系复合膜及补强板,利用环氧胶层黏接PI膜多层结构及氟系聚合物层,利用热膨胀系数小的PI膜作为支撑(若使用小于10ppm/℃的PI膜,可使整体复合PI的热膨胀系数在5~25ppm/c),用来补正氟系树脂高热膨胀系数的不足,使整体结构拥有良好接着强度、低热膨胀系数及高尺寸安定性。由于氟系树脂的高热膨胀系数与PI不匹配造成巨大的热应力,PI与氟系树脂厚度的比率为1~10,厚度比率愈大愈可以减少热应力影响,平坦性越好。The technical problem mainly solved by the present invention is to provide a kind of fluorine-based composite film and reinforcing plate, utilize epoxy adhesive layer to bond PI film multilayer structure and fluorine-based polymer layer, utilize PI film with small coefficient of thermal expansion as support (if The use of PI film less than 10ppm/℃ can make the thermal expansion coefficient of the overall composite PI 5~25ppm/c), which is used to correct the lack of high thermal expansion coefficient of fluororesin, so that the overall structure has good bonding strength, low thermal expansion coefficient and high Dimensional stability. Due to the mismatch between the high thermal expansion coefficient of fluororesin and PI, huge thermal stress is caused. The thickness ratio of PI to fluororesin is 1 to 10. The larger the thickness ratio, the less the influence of thermal stress and the better the flatness.
为解决上述技术问题,本发明采用的一个技术方案是:一种氟系复合膜,包括氟系聚合物层、环氧胶层和聚酰亚胺层;In order to solve the above-mentioned technical problems, a technical solution adopted by the present invention is: a fluorine-based composite film, including a fluorine-based polymer layer, an epoxy adhesive layer and a polyimide layer;
所述环氧胶层的厚度为5-50μm;The thickness of the epoxy adhesive layer is 5-50 μm;
所述氟系聚合物层的厚度为5-125μm;The thickness of the fluoropolymer layer is 5-125 μm;
所述聚酰亚胺层的厚度为5-75μm。The thickness of the polyimide layer is 5-75 μm.
进一步地说,所述氟系复合膜为单面氟系复合膜,所述单面氟系复合膜由上至下依次为氟系聚合物层、聚酰亚胺层、至少一层环氧胶层和至少一层聚酰亚胺层。Furthermore, the fluorine-based composite film is a single-sided fluorine-based composite film, and the single-sided fluorine-based composite film consists of a fluorine-based polymer layer, a polyimide layer, and at least one layer of epoxy glue from top to bottom. layer and at least one polyimide layer.
进一步地说,所述氟系复合膜为双面氟系复合膜,所述双面氟系复合膜由上至下依次为氟系聚合物层、至少一层聚酰亚胺层、至少一层环氧胶层、聚酰亚胺层和氟系聚合物层。Further, the fluorine-based composite film is a double-sided fluorine-based composite film, and the double-sided fluorine-based composite film is sequentially composed of a fluorine-based polymer layer, at least one polyimide layer, at least one layer Epoxy adhesive layer, polyimide layer and fluoropolymer layer.
进一步地说,所述氟系聚合物层中的氟系树脂选自聚四氟乙烯、聚偏氟乙烯、氟乙烯与乙烯基醚共聚物、四氟乙烯与乙烯的共聚物、聚三氟氯乙烯与乙烯共聚物、四氟乙烯、六氟丙烯与偏氟乙烯共聚物、四氟乙烯-全氟烷基乙烯基醚共聚物、聚三氟氯乙烯、聚氯乙烯、四氟乙烯-六氟丙稀共聚物、乙烯-氟乙烯共聚物及四氟乙烯-六氟丙烯-三氟乙烯共聚物中的至少一种。Further, the fluorine resin in the fluorine polymer layer is selected from polytetrafluoroethylene, polyvinylidene fluoride, copolymer of vinyl fluoride and vinyl ether, copolymer of tetrafluoroethylene and ethylene, polychlorotrifluoro Ethylene and ethylene copolymer, tetrafluoroethylene, hexafluoropropylene and vinylidene fluoride copolymer, tetrafluoroethylene-perfluoroalkyl vinyl ether copolymer, polychlorotrifluoroethylene, polyvinyl chloride, tetrafluoroethylene-hexafluoroethylene At least one of propylene copolymer, ethylene-fluoroethylene copolymer, and tetrafluoroethylene-hexafluoropropylene-trifluoroethylene copolymer.
更进一步地说,所述单面氟系复合膜通过烧结法生成的制备方法包括以下步骤:Furthermore, the preparation method of the single-sided fluorine-based composite film by sintering method includes the following steps:
步骤一、将所述氟系聚合物层涂布于所述聚酰亚胺层,于280℃以上进行烧结,得到半成品A;Step 1. Coating the fluorine-based polymer layer on the polyimide layer and sintering above 280°C to obtain a semi-finished product A;
步骤二、将一聚酰亚胺层涂布环氧胶层后,于60-160℃烘烤3~5min去除溶剂,之后贴合半成品A聚酰亚胺层,于160℃烘干固化2h得到成品单面氟系复合膜。Step 2: After coating a polyimide layer with an epoxy adhesive layer, bake it at 60-160°C for 3-5 minutes to remove the solvent, then attach the semi-finished product A polyimide layer, and dry and cure it at 160°C for 2 hours to obtain Finished single-sided fluorine-based composite film.
更进一步地说,若复合膜为不小于六层的2n+4(n为正整数)层结构,所述单面氟系复合膜通过烧结法生成的制备方法包括以下步骤:Furthermore, if the composite membrane has a 2n+4 (n is a positive integer) layer structure of not less than six layers, the preparation method of the single-sided fluorine-based composite membrane generated by sintering method includes the following steps:
步骤一、将所述氟系聚合物层涂布于所述聚酰亚胺层,于280℃以上进行烧结,得到半成品A;Step 1. Coating the fluorine-based polymer layer on the polyimide layer and sintering above 280°C to obtain a semi-finished product A;
步骤二、将一聚酰亚胺层涂布环氧胶层后,于60-160℃烘烤3~5min去除溶剂,贴合于另一聚酰亚胺层上,此步骤重复n次(步骤二、步骤二-2、步骤二-3、.....、步骤二-n);Step 2. After coating a polyimide layer with an epoxy adhesive layer, bake it at 60-160°C for 3 to 5 minutes to remove the solvent, and attach it to another polyimide layer. This step is repeated n times (step Two, step two-2, step two-3, ..., step two-n);
步骤三、将步骤二所得材料涂布环氧胶层,于60-160℃烘烤3~5min去除溶剂,之后贴合半成品A聚酰亚胺层于160℃烘干固化2h,得到单面氟系复合膜。Step 3: Coat the material obtained in Step 2 with an epoxy adhesive layer, bake at 60-160°C for 3-5 minutes to remove the solvent, and then paste the semi-finished product A polyimide layer at 160°C for 2 hours to obtain a single-sided fluorine Department of composite film.
更进一步地说,所述单面氟系复合膜通过贴合法生成的制备方法包括以下步骤:Furthermore, the preparation method of the single-sided fluorine-based composite film by bonding method includes the following steps:
步骤一、将所述聚酰亚胺胶层涂布于所述的氟系聚合物膜,于60-160℃烘烤3~5min去除溶剂,得到半成品A;Step 1. Apply the polyimide adhesive layer on the fluorine-based polymer film, bake at 60-160°C for 3-5 minutes to remove the solvent, and obtain a semi-finished product A;
步骤二、将一聚酰亚胺层涂布环氧胶层后,于60-160℃烘烤3~5min去除溶剂,贴合于另一聚酰亚胺层上;Step 2. After coating a polyimide layer with an epoxy adhesive layer, bake it at 60-160°C for 3-5 minutes to remove the solvent, and attach it to another polyimide layer;
步骤三、将半成品A聚酰亚胺胶层贴合于步骤二所得材料,于160℃烘干固化2h,得到单面氟系复合膜。Step 3: Attach the polyimide adhesive layer of the semi-finished product A to the material obtained in Step 2, and dry and cure at 160°C for 2 hours to obtain a single-sided fluorine-based composite film.
更进一步地说,若复合膜为不小于五层的2n+3(n为正整数)层结构,所述单面氟系复合膜通过贴合法生成的制备方法包括以下步骤:Furthermore, if the composite membrane is not less than five layers of 2n+3 (n is a positive integer) layer structure, the preparation method of the single-sided fluorine-based composite membrane generated by pasting method includes the following steps:
步骤一、将所述聚酰亚胺胶层涂布于所述的氟系聚合物膜,于60-160℃烘烤3~5min去除溶剂,得到半成品A;Step 1. Apply the polyimide adhesive layer on the fluorine-based polymer film, bake at 60-160°C for 3-5 minutes to remove the solvent, and obtain a semi-finished product A;
步骤二、将一聚酰亚胺层涂布环氧胶层后,于60-160℃烘烤3~5min去除溶剂,贴合于另一聚酰亚胺层上,此步骤重复n次(步骤二、步骤二-2、步骤二-3、.....、步骤二-n);Step 2. After coating a polyimide layer with an epoxy adhesive layer, bake it at 60-160°C for 3 to 5 minutes to remove the solvent, and attach it to another polyimide layer. This step is repeated n times (step Two, step two-2, step two-3, ..., step two-n);
步骤三、将半成品A聚酰亚胺胶层贴合于步骤二所得材料,于160℃烘干固化2h,得到单面氟系复合膜。Step 3: Attach the polyimide adhesive layer of the semi-finished product A to the material obtained in Step 2, and dry and cure at 160°C for 2 hours to obtain a single-sided fluorine-based composite film.
更进一步地说,所述双面氟系复合膜通过烧结法生成的制备方法包括以下步骤:Furthermore, the preparation method of the double-sided fluorine-based composite film by sintering method includes the following steps:
步骤一、将所述氟系聚合物层涂布于所述聚酰亚胺层,于280℃以上进行烧结,得到半成品A一与半成品A二;Step 1. Coating the fluorine-based polymer layer on the polyimide layer and sintering above 280° C. to obtain a semi-finished product A1 and a semi-finished product A2;
步骤二、将半成品A一聚酰亚胺层涂布环氧胶层后,于60-160℃烘烤3~5min去除溶剂,之后贴合半成品A二聚酰亚胺层于160℃烘干固化2h,得到双面氟系复合膜;Step 2. After coating the semi-finished product A-polyimide layer with epoxy adhesive layer, bake at 60-160°C for 3-5 minutes to remove the solvent, and then attach the semi-finished product A-dipolyimide layer and dry and cure at 160°C 2h to obtain a double-sided fluorine-based composite film;
更进一步地说,若复合膜部分为不小于七层的2n+5(n为正整数)层结构,所述双面氟系复合膜通过烧结法生成的制备方法包括以下步骤:Furthermore, if the composite membrane part is not less than seven layers of 2n+5 (n is a positive integer) layer structure, the preparation method of the double-sided fluorine-based composite membrane generated by sintering method includes the following steps:
步骤一、将所述氟系聚合物层涂布于所述聚酰亚胺层,于280℃以上进行烧结,得到半成品A一与半成品A二;Step 1. Coating the fluorine-based polymer layer on the polyimide layer and sintering above 280° C. to obtain a semi-finished product A1 and a semi-finished product A2;
步骤二、将半成品A一聚酰亚胺层涂布环氧胶层后,于60-160℃烘烤3~5min去除溶剂,贴合于另一聚酰亚胺层,此步骤重复n次(步骤二、步骤二-2、步骤二-3、.....、步骤二-n);Step 2. After coating the semi-finished product A-polyimide layer with an epoxy adhesive layer, bake it at 60-160°C for 3-5 minutes to remove the solvent, and attach it to another polyimide layer. This step is repeated n times ( Step two, step two-2, step two-3, ..., step two-n);
步骤三、将步骤二所得材料非氟系聚合物层涂布环氧胶层,于60-160℃烘烤3~5min去除溶剂,之后贴合半成品A二聚酰亚胺层于160℃烘干固化2h,得到双面氟系复合膜。Step 3: Coat the non-fluorine-based polymer layer of the material obtained in Step 2 with an epoxy adhesive layer, bake at 60-160°C for 3-5 minutes to remove the solvent, and then paste the semi-finished product A dipolyimide layer and dry at 160°C After curing for 2 hours, a double-sided fluorine-based composite film was obtained.
更进一步地说,所述双面氟系复合膜通过贴合法生成的制备方法包括以下步骤:Furthermore, the preparation method of the double-sided fluorine-based composite film by bonding method includes the following steps:
步骤一、将所述聚酰亚胺胶层涂布于所述的氟系聚合物膜,于60-160℃烘烤3~5min去除溶剂,得到半成品A一与半成品A二;Step 1. Apply the polyimide adhesive layer on the fluorine-based polymer film, bake at 60-160°C for 3-5 minutes to remove the solvent, and obtain semi-finished product A1 and semi-finished product A2;
步骤二、将一聚酰亚胺层涂布环氧胶层后,于60-160℃烘烤3~5min去除溶剂,贴合于另一聚酰亚胺层上;Step 2. After coating a polyimide layer with an epoxy adhesive layer, bake it at 60-160°C for 3-5 minutes to remove the solvent, and attach it to another polyimide layer;
步骤三、将半成品A一与半成品A二的聚酰亚胺胶层分别贴合于步骤二所得材料两面,于160℃烘干固化2h,得到双面氟系复合膜;Step 3: Paste the polyimide adhesive layers of semi-finished product A1 and semi-finished product A2 on both sides of the material obtained in step 2, and dry and cure at 160°C for 2 hours to obtain a double-sided fluorine-based composite film;
更进一步地说,若复合膜部分为不小于七层的2n+5(n为正整数)层结构,所述双面氟系复合膜通过贴合法生成的制备方法包括以下步骤:Furthermore, if the composite membrane part is not less than seven layers of 2n+5 (n is a positive integer) layer structure, the preparation method of the double-sided fluorine-based composite membrane generated by pasting method includes the following steps:
步骤一、将所述聚酰亚胺胶层涂布于所述的氟系聚合物膜,于60-160℃烘烤3~5min去除溶剂,得到半成品A一与半成品A二;Step 1. Apply the polyimide adhesive layer on the fluorine-based polymer film, bake at 60-160°C for 3-5 minutes to remove the solvent, and obtain semi-finished product A1 and semi-finished product A2;
步骤二、将一聚酰亚胺层涂布环氧胶层后,于60-160℃烘烤3~5min去除溶剂,贴合于另一聚酰亚胺层上,此步骤重复n次(步骤二、步骤二-2、步骤二-3、.....、步骤二-n);Step 2. After coating a polyimide layer with an epoxy adhesive layer, bake it at 60-160°C for 3 to 5 minutes to remove the solvent, and attach it to another polyimide layer. This step is repeated n times (step Two, step two-2, step two-3, ..., step two-n);
步骤三、将半成品A一与半成品A二的聚酰亚胺胶层分别贴合于步骤二所得材料两面,于160℃烘干固化2h,得到双面氟系复合膜。Step 3: Paste the polyimide adhesive layers of semi-finished product A1 and semi-finished product A2 on both sides of the material obtained in step 2, and dry and cure at 160°C for 2 hours to obtain a double-sided fluorine-based composite film.
一种氟系补强板,所述氟系补强板由上至下依次为氟系聚合物层、聚酰亚胺层、至少一层环氧胶层、至少一层聚酰亚胺层、环氧胶层和离型层。A fluorine-based reinforcing plate, the fluorine-based reinforcing plate is sequentially composed of a fluorine-based polymer layer, a polyimide layer, at least one epoxy adhesive layer, at least one polyimide layer, Epoxy adhesive layer and release layer.
所述离型层可以是离型膜,其材料为聚丙烯、双向拉伸聚丙烯和聚对苯二甲酸乙二醇酯中的至少一种,且可以是具双面离型能力的离型膜,又或是使用离型纸。The release layer can be a release film whose material is at least one of polypropylene, biaxially oriented polypropylene and polyethylene terephthalate, and can be a release film with double-sided release capability. film, or use release paper.
进一步地说,所述氟系补强板通过烧结法生成的制备方法包括以下步骤:Further, the preparation method of the fluorine-based reinforcing plate through sintering method includes the following steps:
将烧结法制备的单面氟系复合膜非氟系聚合物层涂布环氧胶层后,于60-160℃烘烤3~5min去除溶剂,之后贴合离型层于160℃烘干固化2h,即得成品氟系补强板。After the non-fluorine polymer layer of the single-sided fluorine-based composite film prepared by the sintering method is coated with an epoxy adhesive layer, it is baked at 60-160°C for 3-5 minutes to remove the solvent, and then the release layer is attached and dried at 160°C for curing After 2 hours, the finished fluorine-based reinforced board is obtained.
进一步地说,所述氟系补强板通过贴合法生成的制备方法包括以下步骤:Furthermore, the preparation method of the fluorine-based reinforcing plate produced by bonding method includes the following steps:
将贴合法制备的单面氟系复合膜非氟系聚合物层涂布环氧胶层后,于60-160℃烘烤3~5min去除溶剂,之后贴合离型层于160℃烘干固化2h,即得成品氟系补强板。After coating the non-fluorine polymer layer of the single-sided fluorine-based composite film prepared by lamination method with an epoxy adhesive layer, bake it at 60-160°C for 3-5 minutes to remove the solvent, and then attach the release layer and dry it at 160°C for curing After 2 hours, the finished fluorine-based reinforced board is obtained.
本发明的有益效果:具备良好的尺寸安定性、高耐磨性、超低吸水率、极佳的机械性能、高接着强度等优势。The beneficial effect of the present invention: it has the advantages of good dimensional stability, high wear resistance, ultra-low water absorption, excellent mechanical properties, high bonding strength and the like.
附图说明Description of drawings
图1是本发明单面氟系复合膜、双面氟系复合膜和氟系补强板的结构示意图(烧结法);Fig. 1 is the structural representation (sintering method) of single-sided fluorine-based composite membrane, double-sided fluorine-based composite membrane and fluorine-based reinforcing plate of the present invention;
图2是本发明单面氟系复合膜、双面氟系复合膜和氟系补强板的结构示意图(贴合法);Fig. 2 is the structural representation of single-sided fluorine-based composite film, double-sided fluorine-based composite film and fluorine-based reinforcing plate of the present invention (pasting method);
图3是本发明单面氟系复合膜通过烧结法生成的流程图;Fig. 3 is the flow chart that single-sided fluorine-based composite film of the present invention is produced by sintering method;
图4是本发明双面氟系复合膜通过烧结法生成的流程图;Fig. 4 is the flow chart that double-sided fluorine-based composite film of the present invention is produced by sintering method;
图5是本发明氟系补强板通过烧结法生成的流程图;Fig. 5 is a flow chart of the fluorine-based reinforcing plate of the present invention produced by the sintering method;
图6是本发明单面氟系复合膜通过贴合法生成的流程图;Fig. 6 is a flow chart of the single-sided fluorine-based composite film of the present invention generated by pasting;
图7是本发明双面氟系复合膜通过贴合法生成的流程图;Fig. 7 is a flow chart of the double-sided fluorine-based composite film of the present invention generated by pasting;
图8是本发明氟系补强板通过贴合法生成的流程图;Fig. 8 is a flow chart of the fluorine-based reinforcing plate of the present invention produced by pasting;
附图标记如下:The reference signs are as follows:
氟系复合膜100Fluorine composite film 100
氟系补强板200Fluorine reinforced plate 200
氟系聚合物层101、聚酰亚胺层102、环氧胶层103、聚酰亚胺胶层104和离型层201
具体实施方式Detailed ways
下面结合附图对本发明的较佳实施例进行详细阐述,以使本发明的优点和特征能更易于被本领域技术人员理解,从而对本发明的保护范围做出更为清楚明确的界定。The preferred embodiments of the present invention will be described in detail below in conjunction with the accompanying drawings, so that the advantages and features of the present invention can be more easily understood by those skilled in the art, so as to define the protection scope of the present invention more clearly.
实施例:一种氟系复合膜100,包括氟系聚合物层101、环氧胶层103和聚酰亚胺层102;Embodiment: a fluorine-based composite film 100, including a fluorine-based
所述环氧胶层的厚度为5-50μm;优选15-30μm;The thickness of the epoxy adhesive layer is 5-50 μm; preferably 15-30 μm;
所述氟系聚合物层的厚度为5-125μm;优选5-50μm;The thickness of the fluoropolymer layer is 5-125 μm; preferably 5-50 μm;
所述聚酰亚胺层的厚度为5-75μm;优选12.5-50μm。The thickness of the polyimide layer is 5-75 μm; preferably 12.5-50 μm.
如图1-A和图2-A所示,所述氟系复合膜为单面氟系复合膜,所述单面氟系复合膜由上至下依次为氟系聚合物层、聚酰亚胺层、至少一层环氧胶层和至少一层聚酰亚胺层。As shown in Figure 1-A and Figure 2-A, the fluorine-based composite film is a single-sided fluorine-based composite film, and the single-sided fluorine-based composite film is sequentially composed of a fluorine-based polymer layer, a polyimide An amine layer, at least one epoxy glue layer and at least one polyimide layer.
如图1-B和图2-B所示,所述氟系复合膜为双面氟系复合膜,所述双面氟系复合膜由上至下依次为氟系聚合物层、至少一层聚酰亚胺层、至少一层环氧胶层、聚酰亚胺层和氟系聚合物层。As shown in Figure 1-B and Figure 2-B, the fluorine-based composite film is a double-sided fluorine-based composite film, and the double-sided fluorine-based composite film is a fluorine-based polymer layer from top to bottom, at least one layer A polyimide layer, at least one epoxy adhesive layer, a polyimide layer and a fluoropolymer layer.
所述氟系聚合物层中的氟系树脂选自聚四氟乙烯、聚偏氟乙烯、氟乙烯与乙烯基醚共聚物、四氟乙烯与乙烯的共聚物、聚三氟氯乙烯与乙烯共聚物、四氟乙烯、六氟丙烯与偏氟乙烯共聚物、四氟乙烯-全氟烷基乙烯基醚共聚物、聚三氟氯乙烯、聚氯乙烯、四氟乙烯-六氟丙稀共聚物、乙烯-氟乙烯共聚物及四氟乙烯-六氟丙烯-三氟乙烯共聚物中的至少一种。所述氟系聚合物层中的氟系树脂不限于现有技术外购采用或使用自有技术烧结得出。The fluorine resin in the fluorine polymer layer is selected from polytetrafluoroethylene, polyvinylidene fluoride, copolymer of vinyl fluoride and vinyl ether, copolymer of tetrafluoroethylene and ethylene, copolymer of polychlorotrifluoroethylene and ethylene Tetrafluoroethylene, hexafluoropropylene and vinylidene fluoride copolymer, tetrafluoroethylene-perfluoroalkyl vinyl ether copolymer, polychlorotrifluoroethylene, polyvinyl chloride, tetrafluoroethylene-hexafluoropropylene copolymer , at least one of ethylene-fluoroethylene copolymer and tetrafluoroethylene-hexafluoropropylene-trifluoroethylene copolymer. The fluorine-based resin in the fluorine-based polymer layer is not limited to being purchased from the prior art or obtained by sintering using the own technology.
所述氟系聚合物层可使用烧结法和贴合法生成,烧结法是将氟系聚合物涂布于聚酰亚胺层表面于280℃以上进行烧结得到,厚度为5-50μm;贴合法是将PTFE膜涂布聚酰亚胺胶层贴合与聚酰亚胺层得到,厚度为25-125μm。The fluorine-based polymer layer can be produced by sintering and pasting methods. The sintering method is obtained by coating the fluorine-based polymer on the surface of the polyimide layer and sintering at a temperature above 280° C., with a thickness of 5-50 μm; the pasting method is The PTFE film is coated with a polyimide adhesive layer and laminated with a polyimide layer, and the thickness is 25-125 μm.
所述单面氟系复合膜通过烧结法生成的制备方法包括以下步骤:The preparation method of the single-sided fluorine-based composite film generated by the sintering method comprises the following steps:
步骤一、将所述氟系聚合物层涂布于所述聚酰亚胺层,于280℃以上进行烧结,得到半成品A;Step 1. Coating the fluorine-based polymer layer on the polyimide layer and sintering above 280°C to obtain a semi-finished product A;
步骤二、将一聚酰亚胺层涂布环氧胶层后,于60-160℃烘烤3~5min去除溶剂,之后贴合半成品A聚酰亚胺层,于160℃烘干固化2h得到成品单面氟系复合膜。Step 2: After coating a polyimide layer with an epoxy adhesive layer, bake it at 60-160°C for 3-5 minutes to remove the solvent, then attach the semi-finished product A polyimide layer, and dry and cure it at 160°C for 2 hours to obtain Finished single-sided fluorine-based composite film.
如图3所示,若复合膜为不小于六层的2n+4(n为正整数)层结构,所述单面氟系复合膜通过烧结法生成的制备方法包括以下步骤:As shown in Figure 3, if the composite film is not less than six layers of 2n+4 (n is a positive integer) layer structure, the preparation method of the single-sided fluorine-based composite film generated by sintering method includes the following steps:
步骤一、将所述氟系聚合物层涂布于所述聚酰亚胺层,于280℃以上进行烧结,得到半成品A;Step 1. Coating the fluorine-based polymer layer on the polyimide layer and sintering above 280°C to obtain a semi-finished product A;
步骤二、将一聚酰亚胺层涂布环氧胶层后,于60-160℃烘烤3~5min去除溶剂,贴合于另一聚酰亚胺层上,此步骤重复n次(步骤二、步骤二-2、步骤二-3、.....、步骤二-n);Step 2. After coating a polyimide layer with an epoxy adhesive layer, bake it at 60-160°C for 3 to 5 minutes to remove the solvent, and attach it to another polyimide layer. This step is repeated n times (step Two, step two-2, step two-3, ..., step two-n);
步骤三、将步骤二所得材料涂布环氧胶层,于60-160℃烘烤3~5min去除溶剂,之后贴合半成品A聚酰亚胺层于160℃烘干固化2h,得到单面氟系复合膜。Step 3: Coat the material obtained in Step 2 with an epoxy adhesive layer, bake at 60-160°C for 3-5 minutes to remove the solvent, and then paste the semi-finished product A polyimide layer at 160°C for 2 hours to obtain a single-sided fluorine Department of composite film.
所述单面氟系复合膜通过贴合法生成的制备方法包括以下步骤:The preparation method of the single-sided fluorine-based composite film produced by pasting method comprises the following steps:
步骤一、将所述聚酰亚胺胶层104涂布于所述的氟系聚合物膜,于60-160℃烘烤3~5min去除溶剂,得到半成品A;Step 1. Coating the
步骤二、将一聚酰亚胺层涂布环氧胶层后,于60-160℃烘烤3~5min去除溶剂,贴合于另一聚酰亚胺层上;Step 2. After coating a polyimide layer with an epoxy adhesive layer, bake it at 60-160°C for 3-5 minutes to remove the solvent, and attach it to another polyimide layer;
步骤三、将半成品A聚酰亚胺胶层贴合于步骤二所得材料,于160℃烘干固化2h,得到单面氟系复合膜。Step 3: Attach the polyimide adhesive layer of the semi-finished product A to the material obtained in Step 2, and dry and cure at 160°C for 2 hours to obtain a single-sided fluorine-based composite film.
如图6所示,若复合膜为不小于五层的2n+3(n为正整数)层结构,所述单面氟系复合膜通过贴合法生成的制备方法包括以下步骤:As shown in Figure 6, if the composite film is not less than five layers of 2n+3 (n is a positive integer) layer structure, the preparation method of the single-sided fluorine-based composite film generated by pasting method includes the following steps:
步骤一、将所述聚酰亚胺胶层涂布于所述的氟系聚合物膜,于60-160℃烘烤3~5min去除溶剂,得到半成品A;Step 1. Apply the polyimide adhesive layer on the fluorine-based polymer film, bake at 60-160°C for 3-5 minutes to remove the solvent, and obtain a semi-finished product A;
步骤二、将一聚酰亚胺层涂布环氧胶层后,于60-160℃烘烤3~5min去除溶剂,贴合于另一聚酰亚胺层上,此步骤重复n次(步骤二、步骤二-2、步骤二-3、.....、步骤二-n);Step 2. After coating a polyimide layer with an epoxy adhesive layer, bake it at 60-160°C for 3 to 5 minutes to remove the solvent, and attach it to another polyimide layer. This step is repeated n times (step Two, step two-2, step two-3, ..., step two-n);
步骤三、将半成品A聚酰亚胺胶层贴合于步骤二所得材料,于160℃烘干固化2h,得到单面氟系复合膜。Step 3: Attach the polyimide adhesive layer of the semi-finished product A to the material obtained in Step 2, and dry and cure at 160°C for 2 hours to obtain a single-sided fluorine-based composite film.
所述双面氟系复合膜通过烧结法生成的制备方法包括以下步骤:The preparation method of the double-sided fluorine-based composite film generated by the sintering method comprises the following steps:
步骤一、将所述氟系聚合物层涂布于所述聚酰亚胺层,于280℃以上进行烧结,得到半成品A一与半成品A二;Step 1. Coating the fluorine-based polymer layer on the polyimide layer and sintering above 280° C. to obtain a semi-finished product A1 and a semi-finished product A2;
步骤二、将半成品A一聚酰亚胺层涂布环氧胶层后,于60-160℃烘烤3~5min去除溶剂,之后贴合半成品A二聚酰亚胺层于160℃烘干固化2h,得到双面氟系复合膜;Step 2. After coating the semi-finished product A-polyimide layer with epoxy adhesive layer, bake at 60-160°C for 3-5 minutes to remove the solvent, and then attach the semi-finished product A-dipolyimide layer and dry and cure at 160°C 2h to obtain a double-sided fluorine-based composite film;
如图4所示,若复合膜部分为不小于七层的2n+5(n为正整数)层结构,所述双面氟系复合膜通过烧结法生成的制备方法包括以下步骤:As shown in Figure 4, if the composite membrane part is not less than seven layers of 2n+5 (n is a positive integer) layer structure, the preparation method of the double-sided fluorine-based composite membrane generated by the sintering method includes the following steps:
步骤一、将所述氟系聚合物层涂布于所述聚酰亚胺层,于280℃以上进行烧结,得到半成品A一与半成品A二;Step 1. Coating the fluorine-based polymer layer on the polyimide layer and sintering above 280° C. to obtain a semi-finished product A1 and a semi-finished product A2;
步骤二、将半成品A一聚酰亚胺层涂布环氧胶层后,于60-160℃烘烤3~5min去除溶剂,贴合于另一聚酰亚胺层,此步骤重复n次(步骤二、步骤二-2、步骤二-3、.....、步骤二-n);Step 2. After coating the semi-finished product A-polyimide layer with an epoxy adhesive layer, bake it at 60-160°C for 3-5 minutes to remove the solvent, and attach it to another polyimide layer. This step is repeated n times ( Step two, step two-2, step two-3, ..., step two-n);
步骤三、将步骤二所得材料非氟系聚合物层涂布环氧胶层,于60-160℃烘烤3~5min去除溶剂,之后贴合半成品A二聚酰亚胺层于160℃烘干固化2h,得到双面氟系复合膜。Step 3: Coat the non-fluorine-based polymer layer of the material obtained in Step 2 with an epoxy adhesive layer, bake at 60-160°C for 3-5 minutes to remove the solvent, and then paste the semi-finished product A dipolyimide layer and dry at 160°C After curing for 2 hours, a double-sided fluorine-based composite film was obtained.
所述双面氟系复合膜通过贴合法生成的制备方法包括以下步骤:The preparation method of the double-sided fluorine-based composite film produced by pasting method comprises the following steps:
步骤一、将所述聚酰亚胺胶层涂布于所述的氟系聚合物膜,于60-160℃烘烤3~5min去除溶剂,得到半成品A一与半成品A二;Step 1. Apply the polyimide adhesive layer on the fluorine-based polymer film, bake at 60-160°C for 3-5 minutes to remove the solvent, and obtain semi-finished product A1 and semi-finished product A2;
步骤二、将一聚酰亚胺层涂布环氧胶层后,于60-160℃烘烤3~5min去除溶剂,贴合于另一聚酰亚胺层上;Step 2. After coating a polyimide layer with an epoxy adhesive layer, bake it at 60-160°C for 3-5 minutes to remove the solvent, and attach it to another polyimide layer;
步骤三、将半成品A一与半成品A二的聚酰亚胺胶层分别贴合于步骤二所得材料两面,于160℃烘干固化2h,得到双面氟系复合膜;Step 3: Paste the polyimide adhesive layers of semi-finished product A1 and semi-finished product A2 on both sides of the material obtained in step 2, and dry and cure at 160°C for 2 hours to obtain a double-sided fluorine-based composite film;
如图7所示,若复合膜部分为不小于七层的2n+5(n为正整数)层结构,所述双面氟系复合膜通过贴合法生成的制备方法包括以下步骤:As shown in Figure 7, if the composite membrane part is not less than seven layers of 2n+5 (n is a positive integer) layer structure, the preparation method of the double-sided fluorine-based composite membrane generated by pasting method includes the following steps:
步骤一、将所述聚酰亚胺胶层涂布于所述的氟系聚合物膜,于60-160℃烘烤3~5min去除溶剂,得到半成品A一与半成品A二;Step 1. Apply the polyimide adhesive layer on the fluorine-based polymer film, bake at 60-160°C for 3-5 minutes to remove the solvent, and obtain semi-finished product A1 and semi-finished product A2;
步骤二、将一聚酰亚胺层涂布环氧胶层后,于60-160℃烘烤3~5min去除溶剂,贴合于另一聚酰亚胺层上,此步骤重复n次(步骤二、步骤二-2、步骤二-3、.....、步骤二-n);Step 2. After coating a polyimide layer with an epoxy adhesive layer, bake it at 60-160°C for 3 to 5 minutes to remove the solvent, and attach it to another polyimide layer. This step is repeated n times (step Two, step two-2, step two-3, ..., step two-n);
步骤三、将半成品A一与半成品A二的聚酰亚胺胶层分别贴合于步骤二所得材料两面,于160℃烘干固化2h,得到双面氟系复合膜。Step 3: Paste the polyimide adhesive layers of semi-finished product A1 and semi-finished product A2 on both sides of the material obtained in step 2, and dry and cure at 160°C for 2 hours to obtain a double-sided fluorine-based composite film.
一种氟系补强板,所述氟系补强板(如图1-C和如图2-C)由上至下依次为氟系聚合物层、聚酰亚胺层、至少一层环氧胶层、至少一层聚酰亚胺层、环氧胶层和离型层201。A fluorine-based reinforcing plate, the fluorine-based reinforcing plate (as shown in Figure 1-C and Figure 2-C) is composed of a fluorine-based polymer layer, a polyimide layer, and at least one layer of rings from top to bottom. Oxygen adhesive layer, at least one polyimide layer, epoxy adhesive layer and
所述离型层可以是离型膜,其材料为聚丙烯、双向拉伸聚丙烯和聚对苯二甲酸乙二醇酯中的至少一种,且可以是具双面离型能力的离型膜,又或是使用离型纸。The release layer can be a release film whose material is at least one of polypropylene, biaxially oriented polypropylene and polyethylene terephthalate, and can be a release film with double-sided release capability. film, or use release paper.
如图5所示,所述氟系补强板通过烧结法生成的制备方法包括以下步骤:As shown in Figure 5, the preparation method of the fluorine-based reinforcing plate produced by the sintering method includes the following steps:
将烧结法制备的单面氟系复合膜非氟系聚合物层涂布环氧胶层后,于60-160℃烘烤3~5min去除溶剂,之后贴合离型层于160℃烘干固化2h,即得成品氟系补强板。After the non-fluorine polymer layer of the single-sided fluorine-based composite film prepared by the sintering method is coated with an epoxy adhesive layer, it is baked at 60-160°C for 3-5 minutes to remove the solvent, and then the release layer is attached and dried at 160°C for curing After 2 hours, the finished fluorine-based reinforced board is obtained.
如图8所示,所述氟系补强板通过贴合法生成的制备方法包括以下步骤:As shown in Figure 8, the preparation method of the fluorine-based reinforcing plate produced by bonding method includes the following steps:
将贴合法制备的单面氟系复合膜非氟系聚合物层涂布环氧胶层后,于60-160℃烘烤3~5min去除溶剂,之后贴合离型层于160℃烘干固化2h,即得成品氟系补强板。After coating the non-fluorine polymer layer of the single-sided fluorine-based composite film prepared by lamination method with an epoxy adhesive layer, bake it at 60-160°C for 3-5 minutes to remove the solvent, and then attach the release layer and dry it at 160°C for curing After 2 hours, the finished fluorine-based reinforced board is obtained.
表1是本实施例氟系复合膜、补强板与比较例的叠构Table 1 is the stacked structure of the fluorine-based composite membrane, the reinforcing plate and the comparative example in this embodiment
比较例1、2是一般市场销售复合膜产品Comparative examples 1 and 2 are composite film products sold in the general market
比较例3是一般市场销售补强板产品Comparative example 3 is a general market sales reinforcement plate product
表1Table 1
表2是本实施例氟系复合膜、补强板与比较例的物性测试结果Table 2 is the physical property test results of the fluorine-based composite film of the present embodiment, the reinforcing plate and the comparative example
平坦性测试方法:先将氟系复合膜表面贴合SONY公司所生产的纯胶(商品名D3450)制备成补强板。再将补强板裁切为25cm×25cm的尺寸,并于180℃条件下压合至74.5±1μm的3-Layer双面软性铜箔基板上,再以160℃的条件进行熟化,再将各个实施例样品与对照样品置于光滑平面上,静置20分钟后,量测四个边角的翘曲高度,进行平坦度测试。Flatness test method: First, the surface of the fluorine-based composite film is pasted with pure rubber (trade name D3450) produced by SONY Company to prepare a reinforcing plate. Then cut the reinforcement plate into a size of 25cm×25cm, and press it on the 74.5±1μm 3-Layer double-sided flexible copper foil substrate at 180°C, and then cure it at 160°C, and then The samples of each example and the control sample were placed on a smooth plane, and after standing for 20 minutes, the warpage heights of the four corners were measured to perform a flatness test.
耐磨性测试方法:先将测试样片裁切为15cm×10cm的尺寸,再将测试样片固定于耐磨测试仪光滑平台上,使用#0000号钢丝绒,设置为1kg负载,使钢丝绒在测试样片表面进行来回摩擦,直至样片表面产生划痕后终止,产生划痕前摩擦次数即为测试结果(钢丝绒来回摩擦为一次)。Abrasion resistance test method: first cut the test sample to a size of 15cm×10cm, then fix the test sample on the smooth platform of the wear tester, use #0000 steel wool, set it as a load of 1kg, and make the steel wool in the test The surface of the sample piece is rubbed back and forth until scratches occur on the surface of the sample piece, and the number of rubbing times before scratches is the test result (steel wool rubbing back and forth is one time).
表2Table 2
如表2所示,相较于市场销售规格,本发明氟系复合膜/补强板具有更低的吸水率性能,良好的平坦性、尺寸安定性和耐磨性,并且其高硬度能够更好的防刮伤、划伤。氟系复合膜/补强板翘曲高度相对较小,因而具有较佳的平坦性,且随着总厚度增加,平坦性更为明显。氟系复合膜、补强板的最高翘曲高度≤1cm,为超级平坦型补强板。As shown in Table 2, compared with the specifications sold in the market, the fluorine-based composite film/reinforcing plate of the present invention has lower water absorption performance, good flatness, dimensional stability and wear resistance, and its high hardness can be more Good resistance to scratches, scratches. The warp height of the fluorine-based composite film/reinforcement plate is relatively small, so it has better flatness, and the flatness is more obvious as the total thickness increases. The maximum warping height of the fluorine-based composite film and the reinforcing plate is ≤1cm, which is a super flat reinforcing plate.
以上所述仅为本发明的实施例,并非因此限制本发明的专利范围,凡是利用本发明说明书及附图内容所作的等效结构变换,或直接或间接运用在其他相关的技术领域,均同理包括在本发明的专利保护范围内。The above is only an embodiment of the present invention, and does not limit the patent scope of the present invention. All equivalent structural transformations made by using the description of the present invention and the contents of the accompanying drawings, or directly or indirectly used in other related technical fields, are all the same. The theory is included in the patent protection scope of the present invention.
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CN116751392A (en) * | 2023-07-20 | 2023-09-15 | 昆山雅森电子材料科技有限公司 | High-temperature-resistant covering film and preparation method thereof |
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